CN104556216B - A kind of method that adopts non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder - Google Patents
A kind of method that adopts non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder Download PDFInfo
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Abstract
The invention discloses a kind of method that adopts non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder, first anhydrous barium source and anhydrous titanium source are dissolved in anhydrous low-carbon alcohol, stir, through oil bath backflow, non-hydrolysis condensation reaction occurs and obtain precursor sol; After being dried, adding mineralizer and evenly mix, through calcining, washing obtains Barium Titanate nano-powder. The method has the outstanding advantages such as preparation technology is simple, synthesis temperature is low, the cycle is short, crystal grain good dispersion, therefore has broad application prospects.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, be specifically related to a kind of method that adopts non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder.
Background technology
Barium titanate is a kind of important Ca-Ti ore type ferroelectric material, because it has high dielectric constant, and the performances such as good ferroelectric, piezoelectricity, thus become the primary raw material of manufacturing electronic ceramics, be widely used in multilayer ceramic capacitor, thermal resistor etc. Along with electronic component is to development micro-, thin, light direction, require the continuous increase of the number of plies of multilayer ceramic capacitor medium layer and the thickness of dielectric layer to continue to reduce, therefore for preparing, crystallite dimension is little, particle size distribution range is narrow, the demand of the Barium Titanate nano-powder of good dispersion is growing.
The method of preparing at present barium carbonate powder mainly contains solid phase method, hydro-thermal method, coprecipitation, hydrolytic sol-gel process, non-hydrolytic sol-gel process etc. It is high that solid phase method is prepared barium carbonate powder synthesis temperature, and crystal grain is large and particle diameter distribution is wide, easily introduces impurity. Hydro-thermal method need under high pressure be carried out, higher to equipment requirement, makes the method be difficult to promote. When coprecipitation is prepared barium carbonate powder, because the sediment solubility product constant of barium and titanium differs greatly, be difficult to form uniform sediment, and particle easily reunites, particle diameter distributes wide, unstable product quality. Prepare in barium carbonate powder at hydrolytic sol-gel process, generally adopting expensive metal alkoxide or metal inorganic salt is presoma, because different presoma hydrolysis rates there are differences, therefore need the strict process conditions of controlling. The people such as S.B.Deshpande are taking brium carbonate and butyl titanate as He Tai source, barium source, glacial acetic acid, isopropyl alcohol and water are solvent, adopt hydrolytic sol-gel process at 750 DEG C, to synthesize barium carbonate powder and (see JournalofElectroceramics, 15,103-108,2005); The people such as Yao Yanyan adopt hydrolytic sol-gel process; taking expensive barium metal (for synthesize barium alkoxides under the condition of 0 DEG C of water-bath and nitrogen protection with EGME), as barium source, butyl titanate is titanium source, has synthesized barium titanate and (see silicate journal at 150 DEG C; 2004; Vol.32, P751-754), because barium is heavy metal element; and in the Nature, never found the existence of simple substance barium; so method cost of material is high, technology condition complexity is high, is difficult for promoting.
Non-hydrolytic sol-gel process is a kind of wet chemical method that the nineties in last century, France professor Corriu grade proposed, it is characterized in that without metal alkoxide hydrolytic process, and be directly gel by reactant polycondensation. Compared with traditional hydrolyzed collosol-gelatin (HSG) method, the method has not only been simplified technical process, avoid the reunion causing taking water as solvent, the more important thing is that in sol-gel process, being easy to realize atom level evenly mixes, can greatly reduce the synthesis temperature of oxide, aspect the preparation of barium titanate and barium titanate doping powder, have broad application prospects. The people such as ChaoliangMao adopt non-hydrolytic sol-gel process to prepare barium-strontium titanate powder (to see CeramicsInternational, 2008, Vol.34, P45 – 49), its method is that barium acetate is dissolved in acetic acid, butyl titanate is dissolved in ethanol, after mixing, add a certain amount of acetone, it is heated to 10h in 50 DEG C of left and right water-baths and obtain precursor sol, colloidal sol is placed in to the dry 12h of 120 DEG C of baking ovens and obtains dry gel powder, dry gel powder is sintered into barium-strontium titanate powder through 800 DEG C. But because the solvent acetic acid that is used for dissolving barium acetate is strong lewis acid, be easy to the polymerization of catalysis butyl titanate generation homogeneity, be difficult to form heteropolymerization, this is also the basic reason (in xerogel infared spectrum do not detect Ba-O-Ti bonding) of its synthesis temperature up to 800 DEG C. Therefore preparation method's technique of barium carbonate powder is more complicated at present, synthesis temperature is higher, is not suitable for large industrial production and uses.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that raw material sources are extensive, preparation technology is simple, production cost is low, employing non-hydrolytic sol-gel process is prepared Barium Titanate nano-powder.
For solving above technical problem, technical scheme of the present invention is: a kind of method that adopts non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder, comprises following steps:
(1) appropriate anhydrous barium source, low-carbon alcohols are mixed, add thermal agitation and obtain solution A;
(2) appropriate anhydrous titanium source is dissolved in and in low-carbon alcohols, obtains solution B, then solution B is joined in above-mentioned solution A, uniform stirring, obtains transparent mixed liquor C;
(3) mixed liquor C obtains barium titanate precursor sol D after oil bath refluxes, and adds appropriate mineralizer after being dried, through ball milling, and calcining, washing obtains Barium Titanate nano-powder.
Described anhydrous barium source is anhydrous formic acid barium, anhydrous acetic acid barium.
Described anhydrous titanium source is butyl titanate, tetraisopropyl titanate, titanium ethanolate.
The carbon atom number of described low-carbon alcohols is 1 ~ 4.
The concentration of described mixed liquor C is 0.5 ~ 1.0mol/L.
Described oil bath reflux temperature is 100 ~ 180 DEG C, and oil bath return time is 24 ~ 48h.
Described baking temperature is 130 ~ 260 DEG C.
Described mineralizer is potassium vanadate, sodium vanadate.
The mol ratio of mineralizer and barium titanate dry gel powder consumption is 0 ~ 0.04.
Described calcining heat is 550 ~ 650 DEG C.
Above-mentioned reactive chemistry equation is as follows:
The present invention causes non-hydrolysis condensation reaction in non-aqueous system, form Ba-O-Ti heteropolymerization, make the synthesis temperature of Barium Titanate nano-powder be reduced to 650 DEG C, also introduce innovatively alkali metal vanadate as mineralizer simultaneously, make the temperature of non-hydrolytic sol-gel process synthesis of barium titanate nano-powder further be reduced to 550 DEG C, there is the outstanding advantages such as preparation technology is simple, synthesis temperature is low, the cycle is short, crystal grain good dispersion, therefore there is the wide market space.
Brief description of the drawings
Fig. 1 is the process chart that non-hydrolytic sol-gel process is prepared Barium Titanate nano-powder.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1
With anhydrous acetic acid barium (analyzing pure), butyl titanate (analyzing pure) is presoma, taking ethanol (analyzing pure) as dissolving the solvent of anhydrous acetic acid barium and butyl titanate. First, the anhydrous acetic acid barium that takes 0.025mol in glove box is placed in dry conical flask, then adds the alcohol solvent of 40ml, adds thermal agitation. The butyl titanate that measures 0.025mol is dissolved in the ethanol of 16.7ml, is uniformly mixed. He Bei source, titanium source is mixed, continue to stir. Mixed solution is placed in to the oil bath pan of the 100 DEG C 24h that refluxes and obtains barium titanate precursor solution, precursor solution is placed at 130 DEG C dry, dry gel powder is calcined at 650 DEG C, obtain Barium Titanate nano-powder.
Embodiment 2
With anhydrous acetic acid barium (analyzing pure), butyl titanate (analyzing pure) is presoma, taking ethanol (analyzing pure) as dissolving the solvent of anhydrous acetic acid barium and butyl titanate. Prepare barium carbonate powder technological process used and experiment condition identical with embodiment 1, after being just dried, add mineralizer potassium vanadate, the mol ratio of the amount adding and barium titanate dry gel powder amount is 0.01, and after ball milling, through 550 DEG C of calcinings, washing obtains Barium Titanate nano-powder.
Embodiment 3
With anhydrous acetic acid barium (analyzing pure), titanium ethanolate (analyzing pure) is presoma, taking isopropyl alcohol (analyzing pure) as dissolving the solvent of barium acetate and titanium ethanolate. Prepare barium carbonate powder technological process used and experiment condition identical with embodiment 1. Just oil bath temperature is 120 DEG C, backflow 36h, and baking temperature is 150 DEG C, after being dried, adds potassium vanadate mineralizer, and the mol ratio of the amount adding and barium titanate dry gel powder amount is 0.02, and after ball milling, through 600 DEG C of calcinings, washing obtains Barium Titanate nano-powder.
Embodiment 4
With anhydrous acetic acid barium (analyzing pure), butyl titanate (analyzing pure) is presoma, and taking butanols (analyzing pure) as dissolving the solvent of barium acetate, methyl alcohol (analyzing pure) is for dissolving the solvent of butyl titanate. Prepare barium carbonate powder technological process used and experiment condition identical with embodiment 1. Just oil bath temperature is 140 DEG C, backflow 24h, and baking temperature is 170 DEG C, after being dried, adds sodium vanadate mineralizer, and the mol ratio of the amount adding and barium titanate dry gel powder amount is 0.02, and after ball milling, through 600 DEG C of calcinings, washing obtains Barium Titanate nano-powder.
Embodiment 5
With anhydrous acetic acid barium (analyzing pure), tetraisopropyl titanate (analyzing pure) is presoma, and taking ethanol (analyzing pure) as dissolving the solvent of barium acetate, butanols (analyzing pure) is for dissolving the solvent of tetraisopropyl titanate. Prepare barium carbonate powder technological process used and experiment condition identical with embodiment 1. Just oil bath temperature is 160 DEG C, backflow 48h, and baking temperature is 190 DEG C, after being dried, adds potassium vanadate mineralizer, and the mol ratio of the amount adding and barium titanate dry gel powder amount is 0.03, and after ball milling, through 600 DEG C of calcinings, washing obtains Barium Titanate nano-powder.
Embodiment 6
With anhydrous formic acid barium (analyzing pure), tetraisopropyl titanate (analyzing pure) is presoma, taking methyl alcohol (analyzing pure) as dissolving the solvent of barium formate and tetraisopropyl titanate. Prepare barium carbonate powder technological process used and experiment condition identical with embodiment 1. Just oil bath temperature is 160 DEG C, backflow 36h, and baking temperature is 200 DEG C, after being dried, adds sodium vanadate mineralizer, and the mol ratio of the amount adding and barium titanate dry gel powder amount is 0.03, and after ball milling, through 650 DEG C of calcinings, washing obtains Barium Titanate nano-powder.
Embodiment 7
With anhydrous formic acid barium (analyzing pure), butyl titanate (analyzing pure) is presoma, and taking glycerine (analyzing pure) as dissolving the solvent of barium formate, butanols (analyzing pure) is for dissolving the solvent of butyl titanate. Prepare barium carbonate powder technological process used and experiment condition identical with embodiment 1. Just oil bath temperature is 180 DEG C, backflow 24h, and baking temperature is 240 DEG C, after being dried, adds potassium vanadate mineralizer, and the mol ratio of the amount adding and barium titanate dry gel powder amount is 0.03, and after ball milling, through 600 DEG C of calcinings, washing obtains Barium Titanate nano-powder.
Embodiment 8
With anhydrous formic acid barium (analyzing pure), titanium ethanolate (analyzing pure) is presoma, taking glycerine (analyzing pure) as dissolving the solvent of barium formate and titanium ethanolate. Prepare barium carbonate powder technological process used and experiment condition identical with embodiment 1. Just oil bath temperature is 180 DEG C, backflow 36h, and baking temperature is 260 DEG C, after being dried, adds sodium vanadate mineralizer, and the mol ratio of the amount adding and barium titanate dry gel powder amount is 0.04, and after ball milling, through 650 DEG C of calcinings, washing obtains Barium Titanate nano-powder.
Claims (9)
1. adopt non-hydrolytic sol-gel process to prepare a method for Barium Titanate nano-powder, comprise following steps:
(1) appropriate anhydrous barium source, low-carbon alcohols are mixed, add thermal agitation and obtain solution A;
(2) appropriate anhydrous titanium source is dissolved in and in low-carbon alcohols, obtains solution B, then solution B is joined in above-mentioned solution A, uniform stirring, obtains transparent mixed liquor C;
(3) mixed liquor C obtains barium titanate precursor sol D after oil bath refluxes, and adds appropriate mineralizer after being dried, through ball milling, and calcining, washing obtains Barium Titanate nano-powder;
Described mineralizer is potassium vanadate, sodium vanadate.
2. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: described anhydrous barium source is anhydrous formic acid barium, anhydrous acetic acid barium.
3. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: described anhydrous titanium source is butyl titanate, tetraisopropyl titanate, titanium ethanolate.
4. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: the carbon atom number of described low-carbon alcohols is 1 ~ 4.
5. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: the concentration of described mixed liquor C is 0.5 ~ 1.0mol/L.
6. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: the temperature that described oil bath refluxes is 100 ~ 180 DEG C, and the time that oil bath refluxes is 24 ~ 48h.
7. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: described dry temperature is 130 ~ 260 DEG C.
8. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: the mol ratio of mineralizer and barium titanate dry gel powder consumption is 0 ~ 0.04.
9. the method for preparing according to claim 1 Barium Titanate nano-powder, is characterized in that: the temperature of described calcining is 550 ~ 650 DEG C.
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| CN106380195A (en) * | 2016-10-08 | 2017-02-08 | 东北大学 | Bariumtitanate ceramic and preparation method thereof |
| CN106752142A (en) * | 2016-12-16 | 2017-05-31 | 安徽宝恒新材料科技有限公司 | A kind of preparation method of easy cutting stainless steel plate |
| CN110252306B (en) * | 2019-07-19 | 2021-10-29 | 景德镇陶瓷大学 | Recoverable Fe2TiO5Preparation method and application of/C composite visible light catalytic material |
| CN115135606A (en) * | 2020-02-27 | 2022-09-30 | 东南大学 | Method for preparing tetragonal phase barium titanate nano particles |
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| CN102432286A (en) * | 2011-09-02 | 2012-05-02 | 景德镇陶瓷学院 | Aluminum titanate powder prepared by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature and preparation method thereof |
| CN103556224A (en) * | 2013-11-04 | 2014-02-05 | 景德镇陶瓷学院 | Method for preparing zirconium silicate whisker by employing non-hydrolytic sol-gel technology combined with molten-salt growth method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100562520B1 (en) * | 2003-12-18 | 2006-03-22 | 삼성정밀화학 주식회사 | A method for preparation of barium titanate powder for titanium dioxide sol |
| CN1803718A (en) * | 2006-01-12 | 2006-07-19 | 景德镇陶瓷学院 | Method for synthesizing composite oxide powder by non-hydrolytic sol-gel process with alcohol as oxygen donor |
| CN101823762A (en) * | 2010-05-07 | 2010-09-08 | 景德镇陶瓷学院 | Method for preparing aluminum titanate nano powder by non-hydrolytic sol-gel process |
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